Acetone → Ephedrine

HRID 1277348

反応式

HRID 1277348 の反応式
[CH3:1][C@@H:2]([NH:11][CH3:12])[C@@H:3]([OH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.CC(C)=O>C(OCC)(=O)C>[CH3:1][C@H:2]([NH:11][CH3:12])[C@H:3]([OH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 180AcetoneHCID 9457d-Ephedrine

生成物 1

HCID 9294Ephedrine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

The hydroxy acid obtained above, 18.43 g. (0.093 mole) was dissolved in 200 ml. of ethyl acetate with gentle warming and to the solution was addeda solution of 15.04 g. (0.91 mole) of d-ephedrine, [α]578 =(+)11.4 (acetone), in 80 ml. ethyl acetate. The mixture was stirred at room temperature over night during which time a crop of crystals formed, was removed by filtration and air dried to obtain 18.3 g., M.P. 97°-99° C. This material was recrystallized by dissolving itin a minimum amount of hot ethyl acetate and allowing to stand at ambient temperature over night. After three such recrystallizations, 8.9 g. of thed-ephedrine salt of l-4-hydroxy-4-(p-fluorophenyl)butyric acid, M.P. 105.5°-106.5° C. was obtained.

後処理

  1. dissolution(0.093 mole) was dissolved in 200 ml
  2. customformed
  3. customwas removed by filtration and air
  4. customdried
  5. customto obtain 18.3 g
  6. customThis material was recrystallized
  7. dissolutionby dissolving itin a minimum amount of hot ethyl acetate
  8. waitto stand at ambient temperature over night
  9. customAfter three such recrystallizations, 8.9 g

出典と根拠

ORDレコード
ord-a1fc333e629b44b08d53984a6699367a
出典データセット
uspto-grants-1981_07
特許番号
US04277404

関連ノート

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